Manufacture of black wax



75MB "iwf/550.02m?

Nov. 23, 1937.y A. D. DAVID 2,100,070

' MANUFACTURE oF BLACK WAXV Filed vNOV. 19, 1935 m/vms'vs'l?4 @Rl/"ICE METER /r SEPARTOR CHARGE V/scoS/rr l IN. or

BLCK WAX RUN PRODUCT Patented Nov. 23, 1937 UNITED STATES MANUFACTURE F BLACK WAX Aubrey D. David, Clarendon, Pa., assignor to The Petroleum Processes Corporation, Wichita,

Kans.,

a corporation of Kansas Application November 19, 1935, Serial No. 50,523

3 Claims.

'Ihe objects of this invention are to produce a black wax satisfactory for various commercial purposes requiring insulation, water-proofing,

high dielectric strength and other such characteristics and to derive such a product from readily available stocks, at relatively low cost.

These and other desirable objects are attained in the invention herein disclosed by the novel features hereinafter described and broadly covered in the claims.

The drawing accompanying and forming part of the specification illustrates, by way of disclosure, apparatus suitable for carrying Out the process and certain results as accomplished by the invention.

In the drawing referred to, Fig. 1 is a broken part sectional and partly diagrammatic view illustrating apparatus and various connections for carrying out the process.

Fig. 2 is a curve sheet of a typical run.

Briefly, the invention involves the controlled oxidation of wax-containing pertoleum fractions with air. The factors aifecting the quality and characteristics of the finished product, aside from the special chargingl stock used, are time, temperature, pressure and volume of air. By variations of one or more of such factors, different desirable results may be produced.

Any wax-containing petroleum fractions may be used as the base material. Preferably however, the charging stocks are petrolatum or waxes derived from petrolatum. The properties of the initial material influence the character of the iinished product and the charging stocks should accordingly be selected with regard to the character of the product which it is desired to obtain.

The other factors will ordinarily be found Within the following limits:

Time 5 lto 50 hours.

Temperature 300 F. t'o 600 F.

Pressure, atmospheric to 100 lbs. gage.

Air volume, 1A, to 15 cubic feet per gallon charge per hour.

In the form of apparatus illustrated, a shell still 5, is employed, having perforated pipes 6, in the nature of a steam spider in the bottom of the same. Air under pressure is introduced through piping 1, having an orifice meter 8, or

.the like, interposed in the same.

The still may be charged to a level such as indicated at 9. Evolved gases may be run oil at the top through a line I0, to condenser Il, and separator I2. A recording thermometer is indicated at i 3.

In the speciiic example indicated in the chart Fig. 2, 4000 gallons of petrolatum were charged and 3659 gallons of black wax were recovered.

The physical characteristics of the charge and the product were as indicated in the following table:

Charge Product 101 128 F. Green 20. s 405 F. l0

129 F. Shiny black It will be noted from the curves in the chart that there is a regular increase in viscosity with time. 'I'his is a special feature of the process and is a factor in getting the product of desired viscosity. Also, it will be noted that at a period of approximately 30 hours and coincident with viscosities on the order of 130-150 S. U. 210 F., a marked increase in melting point occurs. This is characteristic also in the attainment of the desired quality.

In the example given, the air differentials shown at the foot of .the chart correspond to the following volumes of air per hour:

Derental inches mercury Air cu. it. per hour rrr-rmanita? l'I'hese air volumes are illustrative and may be varied in processing for diierent types of product.

In general, the product is a new material having a definite characteristic appearance and properties. The texture is smooth and ductile. 'I'he color, by proper control, may be varied from brown to true black. In reected light, the surface may vary in appearance from shiny to dull black.

'I'he melting point of the finished product by the A. S. T. M. petrolatum melting point method is increased from 1 F. to 10 F. The Saybolt Universal viscosity may be increased up to 1500 seconds at 210 F. The A. P. I. gravity may be decreased up to 10 A. P. I.

A specic property of the finished material is the low content of organic acidity, which is less than 0.1 mg. KOH as determined by the A. S. T. M. test for neutralization value. The

finished product has only a slight characteristic odor.l

This new product has many industrial uses and can be produced from petrolatum and other wax-containing petroleum fractions at relatively low cost. The operation is one of controlled oxidation, not distillation and the product is a true wax. No solvents or diluents are required and in fact, no mixtures or mixing of any sort. No steam is required and applied heat is only required at the start. The present practice is to heat the charge in a batch still up to about 450 F. and to then blow the air through the mass for say approximately 48 hours more or less, this air maintaining a state of auto-oxidation and keeping the temperature up so there is no need for ring. This is both a factor in the cost and in the generally* uniform character of the product.

The yield is comparatively high, particularly as there are no waste productsthe start is made with an amorphous wax stock and the final product is the black wax, which differs from the original stock in being black, in having a higher viscosity, harder. tougher or lower penetration test and higher melting point. In the controlled oxidation as disclosed, no cracking takes place, no

special oxidizing Yagents are -required and only air is used.

1/4 to 15 cubic feet per hour per gallon of charge over a period of from 5 to 100 hours.

2. Tire process of claim 1, in which the petrolatum is brought to the required temperature by externally applied heat and in which this temperature is thereafter maintained by heat fromV the exothermic reaction resulting from blowing the air through the hot petrolatum;

3. The herein disclosed process of manufacturing black wax which comprises heating petrolatum stock in a conilned state to a temperature on the order of from 300 to 600 F. and forcing a controlled volume of air under pressure through the confined heated mass of from one quarter to fteen cubic feet per gallon of charge over a period of from about ve to one hundred hours and thereby directly converting said petrolatum stock to a smooth ductile wax of permanent black color, of equal or higher melting point, greatly increased viscosity, lower penetration test and low acidity.

' AUBREY D. DAVID. 

